CN106245071B - Acid non-cyanide plating cadmium additive, plating solution prepares and electroplating technology - Google Patents
Acid non-cyanide plating cadmium additive, plating solution prepares and electroplating technology Download PDFInfo
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- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
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Abstract
It is prepared the invention discloses acid non-cyanide plating cadmium additive, plating solution and electroplating technology, plating solution each component is as follows：35~40g/L of caddy, 140~180g/L of potassium chloride, 120~160g/L of complexant, 1.5~2.5mL/L of brightener, 25~35mL/L of adjuvant；Electroplating manipulation condition is：15~35 DEG C of coating bath temperature, 0.5~1.5A/dm of cathode-current density2, the ratio between cathode and annode area are 2:1, anode has two kinds of materials of cadmium plate and plating high-density graphite plate.Advantages of the present invention mainly has：Brightener and adjuvant are prepared by using high-performance electroplating additive intermediate, polynary complex ion is generated using combination complexant and cadmium ion, improves plating solution performance and coating performance；This technique bath stability, convenient for safeguarding, current efficiency is higher, and covering power is strong, and coating brittleness is small, and corrosion resisting property is good, and properties meet aerospace industry ministerial standard QJ 453 1988《Cadmium plating layer technical conditions》Requirement, electroplating wastewater processing result meets GB 21,900 2008《Pollutant emission standard is electroplated》The requirement of table 3.
Description
Technical field
The present invention relates to field of electroplating, particularly relate to acid non-cyanide plating cadmium additive, plating solution prepares and electroplating technology.
Background technology
Cadmium plating layer has excellent corrosion resistance and flexibility, is once widely used.Cadmium and its compound have
Certain toxicity, at the end of the 20th century, cadmium plating technique has been eliminated in product for civilian use plating substantially, but due to aerospace, navigation and
The particularity requirement of some electronic products, some enterprises also retain a certain amount of cadmium plating technique at present.Traditional cyanide cadmium is molten
Liquid and product quality are stablized, but cyanide is that country forbids strictly one of pollutant used, cyaniding is replaced to plate with non-cyanide plating cadmium
Cadmium is imperative, and it is pressed for time.China carried out non-cyanide plating cadmium some researchs, but relatively fewer.Alkaline non-cyanide
Cadmium plating includes making the cadmium plating technique of complexant with triethanolamine and nitrilotriacetic acid and making the cadmium plating technique of complexant with HEDP[1-2]。
Triethanolamine cadmium plating there are bath stability it is poor the problem of, there are current efficiency is low and wastewater treatment difficulty etc. is asked for HEDP cadmium plating
Topic, therefore both techniques yet there are no the production application of scale.Acid non-cyanide plating cadmium technique has put into industrialized production[3-6],
But it needs to add ethylenediamine tetra-acetic acid and ammonium chloride in plating solution, very big difficulty is brought to electroplating wastewater processing[7], make its application by
Limitation is arrived.
According to National Development and Reform Commission《Industry restructuring catalogue (revision in 2011)》Requirement, National Guizhou Aviation
Aerospace enterprise group eliminate the work of cyanide cadmium technique, uses the acid non-cyanide plating cadmium technique containing EDTA at present, but plate
There is floating phenomenon, and electroplating wastewater cadmium is exceeded after layer olive passivation.At the invitation of Guiyang Surface Engineering employer's organization,
Guangzhou Chao Bang Chemical Co., Ltd.s have carried out the developmental research of non-cyanide plating cadmium technique.
Wherein bibliography：
[1] Wu Load is prosperous, Xue Yongfei, Lu Yamei, waits discussion [J] material protections of alkaline non-cyanide cadmium plating techniques, and 1974,15
(6)：1-9；
[2] Zhang Yuncheng, Hu Runan, to flourish plating handbook [M] Beijing：National Defense Industry Press, 1997：279；
[3] non-cyanide platings of the Yang Feng pavilions using DPE- Ш as additive corrodes every [J] packs, 1983,12 (4)：5-8；
[4] Yang Qinjian non-cyanide platings cadmium is in application [J] plating of our factory and environmental protection, 1996,16 (2)：29-30；
[5] Huangping, Chen Duan outstanding person non-cyanide plating cadmium technical studies and application [J] New Technologies, 2008,30 (11)：17-
18；
[6] Wan Binghua, Yang Jun, Wang Fuxin wait the research of non-cyanide plating cadmiums process exploitation and application [J] plating and finish,
2014,36 (3)：22-25+46；
[7] Yang Qianfang, Feng Shuying, Liu Fang non-cyanide plating cadmium waste water treatment research [J] Sichuan environment, 1982,4 (1)：36-
39。
Invention content
The purpose of the present invention is to propose to acid non-cyanide plating cadmium additive, plating solution prepares and electroplating technology, to solve current nothing
Cyanogen cadmium plating plating solution and quality of coating are poor and the problems such as electroplating wastewater processing is difficult.
The technical proposal of the invention is realized in this way：
Acid non-cyanide plating cadmium additive, including following each component：Complexant, brightener, adjuvant.
The complexant includes tri- kinds of components of A, B, C, and wherein component A includes nitrilotriacetic acid, and B component includes citric acid, wine
Any one in stone acid, gluconic acid, malic acid or two kinds, component C include malonic acid, butadiene dilute acid, the dilute diacid of anti-fourth,
Described tri- kinds of components of A, B, C are uniformly mixed to obtain the complexant by any one in oxalic acid or two kinds.
More preferably, the complexant is added in container in following ratio and is uniformly mixed：A, 300~400g, B, 300~
500g, C, 200~400g.
The brightener includes tri- kinds of components of D, E, F, and wherein D components include α-vinyl-N- propane sulfonic acid yl pyridines inner salts
(CAS NO.6613-64-5), component E include Vanillin, Veratraldehyde, 4- methoxyl groups
Any one in benzaldehyde or two kinds, F components include propine alcohol ethoxy ether, propilolic alcohol propoxyl group ether, N, N- diethyl third
Ynamine, N, N- diethylpropynyl amine formate, N, any one in N- diethyl propargylamine sulfate or two kinds, by D, E, F
Three kinds of components, which are dissolved in, obtains the brightener in isopropanol and water mixed solution.
More preferably, the brightener is prepared in following ratio and method：It is equal that the mixing of 300mL isopropanols is added in 400mL water
It is even, D 30~80g of component are added in, component E 30~50g, F 60~100g of component is stirred to component E and is completely dissolved, benefit adds water to
1000mL。
The adjuvant includes water-soluble polyacrylamide, 2- ethylhexylsulfates sodium salt, N, N, (the 2- hydroxypropyls of N- tri-
Base)-N'- hydroxyethyl ethylenediamine, G components and a kind of condensation product being made of ethylenediamine, dimethyl propylamine and epoxychloropropane,
The G components are consistent with the F components in the brightener.
More preferably, the adjuvant is prepared in following ratio and method：50~80g IC, 113 water-soluble polypropylene acyls
Amine, 20~50g ethylenediamines and dimethyl propylamine and epichlorohydrin condensate, 30~80g 2- ethylhexylsulfates sodium salt,
(2- the hydroxypropyls)-N'- hydroxyethyl ethylenediamine of 10~30g N, N, N- tri- and 30~60g G components are added in 700g water, stirring
Make its dissolving, then mend and add water to 1000mL.113 water-soluble polyacrylamides of IC are by Bluclad S.R.L. suppliers
It provides.
The preparation method of acid non-cyanide plating cadmium solution, step are as follows：
(a) water of the addition 4/5 into coating bath is calculated by plating solution volume, sequentially adds sodium hydroxide, potassium chloride, complexant,
The mass ratio of sodium hydroxide and complexant is 1:2, stirring dissolves above-mentioned substance；
(b) and then caddy is added in, and stirred to dissolving, filter plating solution；
(c) brightener, adjuvant are sequentially added, plating is adjusted for 10% sodium hydroxide solution with dilute hydrochloric acid or mass fraction
Between the pH of liquid to 6.0~7.0, defined volume is added water to, in 0.1A/dm21~8h is electrolysed under current density；
Potassium chloride concentration reaches 140~180g/L in last plating solution, and coordination agent concentration reaches 120~160g/L, caddy
Concentration reaches 32~40g/L, and brightener concentration reaches 1.5~2.5mL/L, and adjuvant concentration reaches 25~35mL/L.
Acid non-cyanide plating cadmium technique, step are as follows：
(1) unplated piece pre-treatment；
(2) acid non-cyanide plating cadmium solution is prepared；
(3) it is electroplated, coating bath temperature is 15~35 DEG C during plating, and cathode-current density is 0.5~1.5A/dm2。
Further, the ratio between cathode and annode area are 2:1, anode is used for the cadmium plate of cadmium content >=99.97% and plating
The area ratio of high-density graphite plate, the cadmium plate and graphite cake is 1:1~1:2.
Beneficial effects of the present invention are：Brightener and auxiliary are prepared using function admirable and the smaller intermediate of adsorptivity
Agent reduces the inclusion content of coating, improves the flexibility and corrosion resistance of coating, polynary using combination complexant and cadmium ion generation
Complex ion makes cadmium ion reach preferable sedimentation potential, improves the covering power and covering power of plating solution, is fitted using coordination ability
In complexing agent cadmium ion, reduce cadmium plating wastewater treatment difficulty, the plating solution and coating performance is made to meet space flight work
Industry ministerial standard QJ 453-1988《Cadmium plating layer technical conditions》Requirement, cadmium plating wastewater treatment result meets GB 21900-2008
《Pollutant emission standard is electroplated》The requirement of table 3.
Specific embodiment
To more fully understand the present invention, make further specific illustrate, but not to the present invention below by following embodiment
Limitation of the invention is can be regarded as, it is nonessential according to some that foregoing invention content is made for those skilled in the art
It improves and adjusts, be also considered as being within the scope of the present invention.
Embodiment 1：
The acidity of the present embodiment is as follows without cyanogen rack plating cadmium plating solution composition and concentration：
Caddy 37g/L, potassium chloride 160g/L, complexant 140g/L, brightener 2mL/L, adjuvant 30mL/L；
Operating condition during plating is as follows：
Coating bath temperature is 15~35 DEG C, and cathode-current density is 0.5~1.5A/dm2, the ratio between cathode and annode area are 2:
1, anode is the area ratio of the cadmium plate of cadmium content >=99.97% and plating high-density graphite plate, the cadmium plate and graphite cake
It is 1:1~1:2.
The complexant is made of tri- kinds of components of A, B, C, and wherein component A is nitrilotriacetic acid, and B component is by citric acid, winestone
The composition of any one or two kinds in acid, gluconic acid, malic acid, component C by malonic acid, butadiene dilute acid, the dilute diacid of anti-fourth,
The composition of any one or two kinds in oxalic acid, complexant are prepared in following ratio：A, 300~400g；B, 300~500g；C、200
~400g is added in container and is uniformly mixed.
The brightener is made of tri- kinds of components of D, E, F, and wherein D components are α-vinyl-N- propane sulfonic acid yl pyridines inner salts
(CAS NO.6613-64-5), component E is by Vanillin, Veratraldehyde, 4- methoxybenzenes
Any one in formaldehyde or two kinds of compositions, F components are by propine alcohol ethoxy ether, propilolic alcohol propoxyl group ether, N, N- diethyl third
Ynamine, N, N- diethylpropynyl amine formate, N, any one or two kinds in N- diethyl propargylamine sulfate are into being grouped as.
Brightener is prepared in following ratio and method：It adds in 300mL isopropanols in 400mL water to be uniformly mixed, by tri- kinds of components of D, E and F
It is dissolved in isopropanol and water mixed liquid by 30~80g, 30~50g and 60~100g respectively, adds water to 1000mL.
The adjuvant is prepared by following methods：50~80g IC, 113 water-soluble polyacrylamides, 20~50g are by second
Condensation product, 30~80g 2- ethylhexylsulfates sodium salt, the 10~30g of diamines, dimethyl propylamine and epoxychloropropane composition
(2- the hydroxypropyls)-N'- hydroxyethyl ethylenediamine of N, N, N- tri- and 30~60g G components (G components and the F components one in brightener
Cause) it adds in 700g water, it stirs to dissolve, then mend and add water to 1000mL.
The acid non-cyanide plating cadmium solution is prepared by following methods：
(a) water of the addition 4/5 into coating bath is calculated by plating solution volume, sequentially adds sodium hydroxide, potassium chloride, complexant,
The mass ratio of sodium hydroxide and complexant is 1:2, stirring dissolves above-mentioned substance；
(b) and then caddy is added in, and stirred to dissolving, filter plating solution；
(c) brightener, adjuvant are sequentially added, plating is adjusted for 10% sodium hydroxide solution with dilute hydrochloric acid or mass fraction
The pH of liquid to 6.5 adds water to defined volume, in 0.1A/dm21~8h is electrolysed under current density；
Potassium chloride concentration reaches 160g/L in last plating solution, and coordination agent concentration reaches 140g/L, and chlorination cadmium concentration reaches
37g/L, brightener concentration reach 2mL/L, and adjuvant concentration reaches 30mL/L.
The acid plating solution and coating performance and cadmium plating wastewater treatment result without cyanogen rack plating cadmium technique is as follows：
Deposition velocity：In Jk=1A/dm2Lower plating, v=0.33 μm/min；
Current efficiency：In Jk=1A/dm2Lower plating, current efficiency 73%；
Covering power：41%~52%.
Covering power：The iron pipe for being 10mm with internal diameter is electroplated, with 1.0A/dm2Current density plating 30min, Cr VI is low
The ratio between coating length and aperture are 9.2 after chromium chromatic passivation；
Coating corrosion resistance：Steel and iron parts are taken by this technique cadmium plating 30min, it is blunt using the low chromium colorful passivating process of Cr VI
Change, the aging 15min at 60 DEG C, then place more than for 24 hours.According to GB/T 10125-1997《Artificial atmosphere corrosion test salt fog tries
It tests》Neutral salt spray test 2000h is carried out, cadmium plating layer is generated without white rust, than aerospace industry ministerial standard QJ 453-1988《Cadmium plating layer
Technical conditions》High 20 times of requirement of 96h neutral salt spray tests or more.
Cadmium plating wastewater treatment：The plating cadmium waste water sodium dimethyl dithiocarbamate precipitates cadmium ion, cadmium after processing
The mass concentration of ion is 0.005mg/L, meets GB 21900-2008《Pollutant emission standard is electroplated》The requirement of table 3.
Embodiment 2：
The acidity of the present embodiment is as follows without cyanogen barrel plating cadmium plating solution composition and concentration：
Caddy 34g/L, potassium chloride 180g/L, complexant 150g/L, brightener 2mL/L, adjuvant 30mL/L；
Operating condition during plating is as follows：
Coating bath temperature is 15~35 DEG C, and plating tank voltage is 4~7V, and drum rotating speed is 3~5r/min, cathode and annode area
The ratio between be 2:1, anode is the face of cadmium plate+plating high-density graphite plate of cadmium content >=99.97%, the cadmium plate and graphite cake
The ratio between product is 1:1~1:2.
The complexant, brightener and adjuvant preparation method are such as embodiment 1.
The acid non-cyanide plating cadmium solution is prepared by following methods：
(a) water of the addition 4/5 into coating bath is calculated by plating solution volume, sequentially adds sodium hydroxide, potassium chloride, complexant,
The mass ratio of sodium hydroxide and complexant is 1:2, stirring dissolves above-mentioned substance；
(b) and then caddy is added in, and stirred to dissolving, filter plating solution；
(c) brightener, adjuvant are sequentially added, plating is adjusted for 10% sodium hydroxide solution with dilute hydrochloric acid or mass fraction
The pH of liquid to 6.5 adds water to defined volume, in 0.1A/dm21~8h is electrolysed under current density；
Potassium chloride concentration reaches 180g/L in last plating solution, and coordination agent concentration reaches 150g/L, and chlorination cadmium concentration reaches
34g/L, brightener concentration reach 2mL/L, and adjuvant concentration reaches 30mL/L.
The acid plating solution and coating performance and cadmium plating wastewater treatment result without cyanogen barrel plating cadmium technique is as follows：
Deposition velocity：In Jk=1A/dm2Lower plating, v=0.29 μm/min；
Current efficiency：In Jk=1A/dm2Lower plating, current efficiency 68%；
Covering power：48%~67%；
Covering power：The iron pipe for being 10mm with internal diameter is electroplated, with 1.0A/dm2Current density plating 30min, Cr VI is low
The ratio between coating length and aperture are 9.4 after chromium chromatic passivation.
Coating corrosion resistance：Steel and iron parts are taken by this technique cadmium plating 30min, it is blunt using the low chromium colorful passivating process of Cr VI
Change, the aging 15min at 60 DEG C, then place more than for 24 hours.According to GB/T 10125-1997《Artificial atmosphere corrosion test salt fog tries
It tests》Neutral salt spray test 2000h is carried out, cadmium plating layer is generated without white rust, than aerospace industry ministerial standard QJ 453-1988《Cadmium plating layer
Technical conditions》High 20 times of requirement of 96h neutral salt spray tests or more.
Cadmium plating wastewater treatment：The plating cadmium waste water sodium dimethyl dithiocarbamate precipitates cadmium ion, cadmium after processing
The mass concentration of ion is 0.007mg/L, meets GB 21900-2008《Pollutant emission standard is electroplated》The requirement of table 3.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
With within principle, any modification, equivalent replacement, improvement and so on should all be included in the protection scope of the present invention god.
Claims (9)
1. acid non-cyanide plating cadmium additive, which is characterized in that including following each component：Complexant, brightener, adjuvant；
The complexant include tri- kinds of components of A, B, C, wherein component A include nitrilotriacetic acid, B component include citric acid, tartaric acid,
Any one in gluconic acid, malic acid or two kinds, component C include malonic acid, maleic acid, fumaric acid, oxalic acid
In any one or two kinds, described tri- kinds of components of A, B, C are uniformly mixed to obtain the complexant；
The brightener includes tri- kinds of components of D, E, F, and wherein D components include α-vinyl-N- propane sulfonic acid yl pyridines inner salts (CAS
NO.6613-64-5), component E includes Vanillin, Veratraldehyde, 4- methoxybenzene first
Any one in aldehyde or two kinds, F components include propine alcohol ethoxy ether, propilolic alcohol propoxyl group ether, N, N- diethyl propargylamines,
N, N- diethylpropynyl amine formate, N, any one in N- diethyl propargylamine sulfate or two kinds, by tri- kinds of groups of D, E, F
Divide to be dissolved in and the brightener is obtained in isopropanol and water mixed solution；
The adjuvant include water-soluble polyacrylamide, 2- ethylhexylsulfates sodium salt, N, N, N- tri- (2- hydroxypropyls)-
N'- hydroxyethyl ethylenediamine, G components and the condensation product being made of ethylenediamine, dimethyl propylamine and epoxychloropropane, the G groups
Divide consistent with the F components in the brightener.
2. acidity non-cyanide plating cadmium additive as described in claim 1, it is characterised in that：The complexant is added in following ratio
It is uniformly mixed in container：A, 300~400g, B, 300~500g, C, 200~400g.
3. acidity non-cyanide plating cadmium additive as described in claim 1, it is characterised in that：The brightener is in following ratio and side
It is prepared by method：300mL isopropanols are added in 400mL water to be uniformly mixed, and add in D 30~80g of component, component E 30~50g, F component 60
~100g, stirs to component E and is completely dissolved, and benefit adds water to 1000mL.
4. acidity non-cyanide plating cadmium additive as described in claim 1, it is characterised in that：The adjuvant in following ratio and
It is prepared by method：50~80g water-soluble polyacrylamides, 20~50g ethylenediamines and dimethyl propylamine and epichlorohydrin condensate,
30~80g 2- ethylhexylsulfates sodium salt, 10~30g N, N, N- tri- (2- hydroxypropyls)-N'- hydroxyethyl ethylenediamine and 30
~60g G components are added in 700g water, are stirred to dissolve, then mend and add water to 1000mL.
5. the preparation method of acid non-cyanide plating cadmium solution, it is characterised in that：It is prepared by following methods：
(a) water of the addition 4/5 into coating bath is calculated by plating solution volume, adds in sodium hydroxide, potassium chloride, complexant, sodium hydroxide
Mass ratio with complexant described in claim 1 is 1:2, stirring dissolves above-mentioned substance；
(b) and then caddy is added in, and stirred to dissolving, filter plating solution；
(c) addition brightener described in claim 1, adjuvant described in claim 1 are with dilute hydrochloric acid or mass fraction
10% sodium hydroxide solution adjusts the pH value of plating solution between 6.0~7.0, defined volume is added water to, in 0.1A/dm2Electricity
1~8h is electrolysed under current density；
Potassium chloride concentration reaches 140~180g/L in the plating solution finally obtained, and coordination agent concentration described in claim 1 reaches
120~160g/L, chlorination cadmium concentration reach 32~40g/L, and brightener concentration described in claim 1 reaches 1.5~2.5mL/
L, adjuvant concentration described in claim 1 reach 25~35mL/L.
6. acid non-cyanide plating cadmium technique, it is characterised in that：
(1) unplated piece pre-treatment；
(2) the acid non-cyanide plating cadmium solution described in claim 5 is prepared；
(3) it is electroplated, coating bath temperature is 15~35 DEG C during plating, and cathode-current density is 0.5~1.5A/dm2。
7. acidity non-cyanide plating cadmium technique as claimed in claim 6, it is characterised in that：
The ratio between cathode and annode area are 2:1.
8. acidity non-cyanide plating cadmium technique as claimed in claim 6, it is characterised in that：
The anode is the cadmium plate of cadmium content >=99.97% and plating graphite cake.
9. acidity non-cyanide plating cadmium technique as claimed in claim 8, it is characterised in that：
The area ratio of the cadmium plate and graphite cake is 1:1~1:2.
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| CN113755910A (en) * | 2021-09-18 | 2021-12-07 | 中国航发北京航空材料研究院 | Cyanide-free electroplating cadmium solution with alkyl glycoside as additive component |
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